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Method for synthesizing vinyl phenyl silicone oil

A technology of vinyl phenyl silicone and a synthesis method, which is applied in the field of synthesis of vinyl phenyl silicone oil, can solve the problems of unreliable storage stability of phenyl silicone oil, yellowish color of phenyl silicone oil, insufficient rearrangement reaction and the like, Achieve high reliability, high transparency, and good reactivity

Active Publication Date: 2010-11-17
东莞市贝特利新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, CN200410018067.4 reported that phenyl silicone oil was catalyzed by tetramethyl ammonium oxide or its silicon alkoxide. Since tetramethyl ammonium hydroxide or its silicon alkoxide could not withstand high temperature, it could only be used at low temperature, but low temperature The rearrangement reaction of siloxane units containing phenyl chain members is not sufficient. Therefore, the storage stability of the synthesized phenyl silicone oil is unreliable, and it is easy to mix. The higher the phenyl content, the more obvious the phenomenon
In addition, the color of phenyl silicone oil synthesized by this method is yellowish, which will affect the luminous flux if it is used in LED packaging

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Take 50 grams of hydroxyl-terminated low-polymerization phenylsiloxane, 30 grams of methylcyclosiloxane, and 5 grams of tetramethyldivinyldisiloxane into a 250-milliliter three-necked glass bottle, stir and heat up to 180°C, when the mixture becomes translucent, add 0.3 g of a saturated aqueous solution of potassium hydroxide, continue stirring for 5 hours, cool to room temperature, add 0.1 g of concentrated hydrochloric acid, continue stirring for 2 hours, then add 1 g of sodium carbonate, Continue to stir for 2 hours, stop stirring, carry out suction filtration on the reaction mixed liquid 3 times, collect the filtrate in a three-necked flask, and remove low boilers in vacuum at 180°C, and finally obtain transparent vinyl phenyl silicone oil with high refractive index ,As shown in Table 1.

Embodiment 2

[0012] Take 50 grams of hydroxyl-terminated low-polymerization phenylsiloxane, 100 grams of methylcyclosiloxane, and 5 grams of tetramethyldivinyldisiloxane into a 250-milliliter three-necked glass bottle, stir and heat up to 150°C, when the mixture becomes translucent, add 0.3 g of a saturated aqueous solution of potassium hydroxide, continue stirring for 5 hours, cool to room temperature, add 0.1 g of concentrated hydrochloric acid, continue stirring for 2 hours, then add 1 g of sodium carbonate, Continue to stir for 2 hours, stop stirring, carry out suction filtration on the reaction mixed liquid 3 times, collect the filtrate in a three-necked flask, and remove low boilers in vacuum at 180°C, and finally obtain transparent vinyl phenyl silicone oil with high refractive index ,As shown in Table 1.

Embodiment 3

[0014] Take 50 grams of phenylsiloxane with a low degree of polymerization terminated by hydroxyl groups, 50 grams of methylcyclosiloxane, and 5 grams of tetramethyldivinyldisiloxane and put them into a 250 ml three-necked glass bottle, stir and heat up to 160°C, when the mixture becomes translucent, add 0.3 g of a saturated aqueous solution of sodium hydroxide, continue stirring for 5 hours, cool to room temperature, add 0.1 g of concentrated hydrochloric acid, continue stirring for 2 hours, then add 1 g of calcium carbonate, Continue to stir for 2 hours, stop stirring, carry out suction filtration on the reaction mixed liquid 3 times, collect the filtrate in a three-necked flask, and remove low boilers in vacuum at 180°C, and finally obtain transparent vinyl phenyl silicone oil with high refractive index ,As shown in Table 1.

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Abstract

The invention discloses a method for synthesizing vinyl phenyl silicone oil. The method comprises the following steps of: A, measuring and placing hydroxyl-terminated low-polymerization degree phenyl siloxane, methyl yclosiloxane, and a vinyl silicone terminating agent into a reaction container; raising the temperature to be between 150 and 180 DEG C; fully stirring until a mixture is semitransparent; adding an alkali catalyst into the mixture; and continuously stirring for 6 to 10 hours to obtain reaction liquid; B, cooling the reaction liquid in the step A to room temperature; adding an acid neutralizer; continuously stirring for 2 to 5 hours; adding a soluble carbonate; and leaching for 2 to 4 times after stirring for 2 to 5 hours to obtain a filtrate; and C, removing low-boiling-point substance from the filtrate of the step B in vacuum at the temperature of between 160 and 180 DEG C; and finally obtaining transparent high-refractive index vinyl phenyl silicone oil. The vinyl phenyl silicone oil synthesized by the method has the characteristics of high refractive index (25 DEG C, 1.54), high transparency, good high-temperature stability and high reactivity.

Description

technical field [0001] The invention relates to a method for synthesizing silicone oil, in particular to a method for synthesizing vinylphenyl silicone oil. Background technique [0002] Vinyl phenyl silicone oil is a basic raw material for LED silicone packaging materials, its quality and technical indicators directly affect the quality of LED lights. At present, there are more or less defects in the preparation methods of some phenyl silicone oils. For example, CN200410018067.4 reported that phenyl silicone oil was catalyzed by tetramethyl ammonium oxide or its silicon alkoxide. Since tetramethyl ammonium hydroxide or its silicon alkoxide could not withstand high temperature, it could only be used at low temperature, but low temperature The rearrangement reaction of siloxane units containing phenyl chain members is not sufficient. Therefore, the storage stability of the synthesized phenyl silicone oil is unreliable, and it is easy to mix. The higher the phenyl content, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06
Inventor 殷永彪汤胜山王全
Owner 东莞市贝特利新材料有限公司
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